CN109825856A - Dendrite nickel catalyst electrode preparation facilities and method based on 3D printing - Google Patents
Dendrite nickel catalyst electrode preparation facilities and method based on 3D printing Download PDFInfo
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- CN109825856A CN109825856A CN201910159965.8A CN201910159965A CN109825856A CN 109825856 A CN109825856 A CN 109825856A CN 201910159965 A CN201910159965 A CN 201910159965A CN 109825856 A CN109825856 A CN 109825856A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses dendrite nickel catalyst electrode preparation facilities and method based on 3D printing, including industrial personal computer (1), chemical pump (2), anode tool-electrode (4), plating solution spray head (5), connector (7), coating bath (8), three-dimensional mobile platform (10)；Industrial personal computer (1) is used as three-dimensional motion control system, and the modeling graph data of the nickel catalyst electrode for receiving user is automatically converted into the motion control data of three-dimensional mobile platform, for controlling three-dimensional mobile platform in X, Y, Z-direction movement.By the flowing of plating solution vertically downward, so that electrode surface is formed pine-tree structure, effectively facilitate the catalysis response area of electrode.
Description
Technical field
The invention belongs to mechanical manufacturing fields, prepare more particularly to a kind of dendrite nickel catalyst electrode based on 3D printing
Device and method.
Background technique
The world today, the fossil fuel that can satisfy energy demand are decayed rapidly, at the same time, the combustion of fossil fuel
Burn the life and health of natural environment and people that environmental problem caused by product is also depended on for existence in progressive failure people.Institute
With efficient, the cheap new energy of exploitation, which becomes, to be had to solve the problems, such as.In the new energy developed, hydrogen as energy source
It is considered as one of the new energy of most excellent application prospect.Currently, in main hydrogen preparation method, electrolysis water liberation of hydrogen energy
The enough hydrogen for directly preparing higher degree, and the energy conversion rate height of electrolytic process is, it can be achieved that mass production.With following each
The progress of kind generation technology and the research and development preparation of the various electrode materials haveing excellent performance, the cost of electrolysis water can be greatly diminished.
Currently, it is industrial it is most important, be also that be known as best electrolysis water liberation of hydrogen catalyst be platinum based catalyst.However, noble metal
Skilful expensive price increases the cost of electrolysis water.Therefore, the efficient electrolysis elutriation that exploitation is cheap, overpotential is low, stability is good
Hydrogen catalyst and electrode material are current research hotspots.
Currently, the preparation method of common metal catalytic material mainly has hydrothermal synthesis method, template and goes both at home and abroad
Alloyage etc..
Hydrothermal synthesis method in closed reactor, is added to mixed solution using aqueous solution or other liquid as solvent
Heat, pressurization, form the reaction environment of certain temperature, pressure, and substance dissolution, reaction, recrystallization is made to form simply having for novel substance
The synthetic method of effect.Very important, hydrothermal synthesis method is more demanding to the seal degree of reaction kettle, exists when air pressure is excessively high
It is potential dangerous.Hydrothermal synthesis experiment generally requires " several determinations ": determining reactant, determines metering ratio, the determination of reactant
The addition sequence of reactant determines reaction temperature, reaction time, and therefore, the factor for influencing product is more, workload often compared with
Greatly.
Template be it is traditional prepare orderly dendritic materials method, there are the spies such as easy to operate, morphology controllable, uniform rule
Point.This method has the advantages that accurately to control pore size and microstructure is periodic, but would generally generate one-dimensional porosity
Material.Dendritic metal is prepared with general applicability, research shows that the method is suitable for the electricity of various metals using template
Deposition, the three-dimensional dendritic metal of preparation all have dominance structure very outstanding, big specific surface area and high porosity, can be fine
Be applied to fuel cell, lithium ion battery, in the fields such as electrochemical capacitor and electro-catalysis, this method feasibility is higher, former
Reason is simple, but because its operating process is cumbersome, and higher cost is without being suitably applied large-scale production.
Alloyage is gone to be usually used in preparing dendritic metal material.The uniform alloy material of structure is made first, then using chemistry
Or electrochemical method dissolution removes more active component, leaves the structure of dendrite.This method can by corrosion process with
And the adjustment of follow-up heat treatment process is realized and is controlled the dynamic of bore hole size and spatial arrangement.But alloyage is gone to need to prepare not
With the alloy of composition, and alloy carries out the pre-processing such as annealing to guarantee the uniformity of alloy structure, and goes alloy mistake
The condition control of journey also drastically influences the structure and form that material is made, and in addition the pre-processing of alloy and removes alloy process
It is a time-consuming process.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of dendrite based on 3D printing in view of the deficiencies of the prior art
Nickel catalyst electrode preparation facilities and method.
Technical scheme is as follows:
A kind of dendrite nickel catalyst electrode preparation facilities based on 3D printing, including industrial personal computer (1), chemical pump (2), anode
Tool-electrode (4), plating solution spray head (5), connector (7), coating bath (8), three-dimensional mobile platform (10)；Industrial personal computer (1) is used as three-dimensional
Kinetic control system, the modeling graph data of the nickel catalyst electrode for receiving user, is automatically converted into three-dimensional mobile platform
Motion control data, for controlling three-dimensional mobile platform in X, Y, Z-direction movement；
Plating solution spray head (5) includes guide pipe (11), perforated baffle (15), nozzle housing body (16)；Wherein nozzle housing body
It (16) is the consistent cylindrical shape of internal diameter, plating solution sprays vertically downward, can form pine-tree structure in electrode surface；Nozzle housing body
(16) upper end is fixed with guide pipe (11), and guide pipe (11) is for sealing and clamping anode tool-electrode (4), perforated baffle (15)
It is mounted on anode tool-electrode (4) by interference connection, load has alloying metal particle (14) on perforated baffle, passes through alloy
Clipped wire (14) supplements the ion consumed in plating solution；It is provided with through-hole in the outer surface on nozzle housing body (16) top, it should
Hole is connected with emulsion tube (3) one end, then emulsion tube (3) other end is connected with chemical pump (2) entrance, chemical pump (2) outlet
It is passed through coating bath (8), plating solution circulates in realization coating bath；Open chemical pump (2) after, plating solution from plating solution spray head vertically downward
Outflow；
Substrate work-piece (9) is lain in coating bath (8), and anode tool-electrode (4) passes through connector together with plating solution spray head (5)
(7) for clamping on three-dimensional mobile platform (10), three-dimensional mobile platform (10) drives anode tool-electrode (4) and plating solution spray head (5)
It moves in three-dimensional space；Anode tool-electrode (4) and substrate work-piece (9) connect industrial personal computer (1) medium-high frequency pulse power respectively
Anode and cathode drive anode tool-electrode (4) and plating solution spray head through three-dimensional mobile platform (10) under the control of industrial personal computer
(5) it is moved according to the motion control data of three-dimensional mobile platform along the track of setting.
The dendrite nickel catalyst electrode preparation facilities, anode tool-electrode (4) have curvature, curvature with it is pre-prepared
Dendrite nickel catalyst electrode skeleton curvature is identical, is acted on by the lower local plating of anode tool-electrode guidance, deposit and
The identical nickel catalyst electrode of anode shape.
The dendrite nickel catalyst electrode preparation facilities, industrial personal computer (1) are real according to the current value to high frequency pulse power supply
When monitor, constantly adjust anode tool-electrode (4) height, the electrode spacing position of anode tool-electrode and preparation made to keep permanent
It is fixed.
The method for preparing dendrite nickel catalyst electrode according to any described device:
Step (1): substrate work-piece (9) is laid flat into coating bath (8), selects be suitble to the anode tool of curvature electric as needed
Pole (4), and be connected with plating solution spray head (5), anode tool-electrode (4) exposes outside nozzle mouth 0.5cm, is being fixed to three
On the connector (7) for tieing up mobile platform (10)；
Step (2): by industrial personal computer (1) medium-high frequency pulse power anode and cathode respectively with anode tool-electrode (4) and base
Body workpiece (9) is connected, and three-dimensional mobile platform z-axis coordinate is adjusted, so that anode tool-electrode (4) is with substrate work-piece (9) surface
The interval 1mm；The inlet of chemical pump (2) is connected with coating bath (8) again, exports the two inlet phase of outside with plating solution spray head (5)
Even, chemical pump (2) are opened, so that flowing to substrate work-piece (9) surface from spray head (5) after plating solution reaches 0.1Mpa pressure；
Step (3): importing the modeling graph data of the nickel catalyst electrode of user in industrial personal computer (1), opens high frequency arteries and veins
Rush power supply, the curent change between industrial personal computer (1) real-time detection anode tool-electrode (4) and the electrode of preparation, when the electricity of generation
When pole and anode tool-electrode (4) spacing are too small, electric current increases, and when being more than set threshold current, controls three-dimensional mobile
Platform is lifted along z-axis, so that electric current maintains always setting value, to guarantee to maintain between anode tool-electrode (4) and component
Suitable interpolar away from.
Step (4): after electrode growth reaches specified size, stop high frequency pulse power supply power supply, stop chemical pump (2) work
Make, substrate work-piece (9) are taken out, flattens use after cutting the electrode of generation.
The method, high frequency pulse power supply output voltage are constant pressure 6V.
The method, suitable interpolar is away between 0.1-1mm between anode tool-electrode (4) and component.
The method, plating solution use: the nickel sulfate of 300g/l, the nickel chloride of 40g/l and the boric acid of 40g/l；First burning
Boric acid and 990mL distilled water are successively poured into cup, 70-90 DEG C of heating water bath simultaneously dissolves boric acid with glass bar stirring；Then it falls
Enter nickel sulfate and nickel chloride, continue heating water bath and is stirred with glass bar to whole dissolutions；Pour into active carbon particle and hydrogen peroxide
Reagent activates 30min, and is filtered for use with filter paper；The distilled water that remaining 10mL is poured into another beaker, with homogenizer with
600-700r/min revolving speed stirs 10min, stands stand-by to room temperature.
Compared with the existing technology, the invention has the following beneficial effects:
1, by high-frequency impulse electro-deposition method, preparation process is simple, efficiently, it can be achieved that the quick increasing material system of nickel base electrode
It makes.
2, plating solution makes electrode surface form pine-tree structure, effectively facilitates urging for electrode by the flowing of plating solution vertically downward
Change response area.
3, Positioning Servo System detects the curent change between anode tool-electrode and electrode, judges sun with this
The distance between pole tool-electrode and electrode, and guarantee to tie up between tool-electrode and workpiece by the movement of control mobile platform
It holds in suitable distance, improves the stability that electrode increases material process.
4, by three-dimensional mobile platform and with the anode tool-electrode for preparing dendrite skeleton same curvature, guided by anode
Under local plating effect, electrode identical with anode shape can be deposited.Anode is arranged to the circular shape with curvature,
The electrode structure with curvature can be prepared, get rid of substrate work-piece size limitation, using 3d printing space advantage, it can be achieved that
Large-scale electrode increasing material manufacturing (as shown in Figure 3), further increases the practical application value of the device.
Detailed description of the invention
Fig. 1 is dendrite nickel catalyst electrode increasing material manufacturing apparatus structure schematic diagram
Fig. 2 is dendrite nickel catalyst electrode increasing material manufacturing device plating solution structural scheme of mechanism
Fig. 3 is that dendrite arm nickel catalyst electrode increases material pictorial diagram
In figure: 1, industrial personal computer, 2, chemical pump, 3, emulsion tube, 4, anode tool-electrode, 5, plating solution spray head, 7, connector, 8,
Coating bath, 9, substrate work-piece, 10, three-dimensional mobile platform, 11, guide pipe, 12, O-ring, 13, metal tube, 14, alloying metal particle,
15, perforated baffle, 16, nozzle housing body.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
As depicted in figs. 1 and 2, a kind of a wide range of novel dendrite nickel catalyst electrode preparation facilities based on 3D printing, packet
Include industrial personal computer 1, chemical pump 2, anode tool-electrode 4, plating solution spray head 5, connector 7, coating bath 8, three-dimensional mobile platform 10；Industrial personal computer
1, which is used as three-dimensional motion control system, is automatically converted into three-dimensional shifting for receiving the modeling graph data of user's nickel catalyst electrode
The motion control data of moving platform, for controlling three-dimensional mobile platform in X, Y, Z-direction movement；
Plating solution spray head 5 includes guide pipe 11, perforated baffle 15, nozzle housing body 16；Wherein nozzle housing body 16 is cylinder
Shape；16 upper end of nozzle housing body is fixed with guide pipe 11, and guide pipe 11 is for sealing and clamping anode tool-electrode 4, porous gear
Plate 15 is mounted on anode tool-electrode 4 by interference connection, and load has alloying metal particle 14 on perforated baffle, passes through alloy
Clipped wire 14 supplements the ion consumed in plating solution；It is provided with through-hole in the outer surface on nozzle housing body top, the hole and cream
3 one end of sebific duct is connected, then 3 other end of emulsion tube is connected with 2 entrance of chemical pump, and the outlet of chemical pump 2 is passed through coating bath 8, realizes
Plating solution circulates in coating bath；After opening chemical pump 2, plating solution flows out straight down from plating solution spray head；
Substrate work-piece 9 is lain in coating bath 8, and anode tool-electrode 4 is together with plating solution spray head 5 by 7 clamping of connector three
It ties up on mobile platform 10, three-dimensional mobile platform 10 drives anode tool-electrode 4 and plating solution spray head 5 to move in three-dimensional space；Sun
Pole tool-electrode 4 and substrate work-piece 9 connect the anode and cathode of the 1 medium-high frequency pulse power of industrial personal computer respectively, mobile flat by three-dimensional
Platform 10 drives anode tool-electrode 4 and plating solution spray head 5 according to the motion control number of three-dimensional mobile platform under the control of industrial personal computer
It is moved according to along the track of setting.
Anode tool-electrode 4 has curvature, and curvature is identical as pre-prepared dendrite nickel catalyst electrode skeleton curvature, passes through
Local plating effect under the guidance of anode tool-electrode, can deposit nickel catalyst electrode identical with anode shape.
Nozzle housing body 16 is the consistent cylinder of internal diameter, such plating solution can ejection vertically downward, be convenient for electrode surface shape
At pine-tree structure.
Industrial personal computer 1 constantly adjusts 4 height of anode tool-electrode according to the current value real-time monitoring to high frequency pulse power supply,
Keep constant the electrode spacing position of anode tool-electrode and preparation.
Plating solution uses: the nickel sulfate of 300g/l, the nickel chloride of 40g/l and the boric acid of 40g/l.First successively poured into beaker
Boric acid and 990mL distilled water, 70-90 DEG C of heating water bath simultaneously dissolve boric acid with glass bar stirring；It is subsequently poured into nickel sulfate and chlorine
Change nickel, continue heating water bath and is stirred with glass bar to whole dissolutions；Pour into active carbon particle and the activation of hydrogen peroxide reagent
30min, and filtered for use with filter paper；The distilled water that remaining 10mL is poured into another beaker, with homogenizer with 600-700r/
Min revolving speed stirs 10min, stands stand-by to room temperature.
The work step of the device is as follows:
Step 1: substrate work-piece 9 is laid flat in coating bath 8, selects the anode tool-electrode 4 for being suitble to curvature as needed, and
It is connected with plating solution spray head 5, anode tool-electrode 4 exposes outside nozzle mouth 0.5cm, is being fixed to three-dimensional mobile platform 10
Connector 7 on.
Step 2: by 1 medium-high frequency pulse power anode of industrial personal computer and cathode respectively with anode tool-electrode 4 and substrate work-piece 9
It is connected, adjusts three-dimensional mobile platform z-axis coordinate, so that anode tool-electrode 4 and 9 surface of substrate work-piece is the interval 1mm.It will change again
The inlet of work pump 2 is connected with coating bath 8, and outlet is connected with two inlet of outside of plating solution spray head 5, opens chemical pump 2, so that plating
After liquid reaches 0.1Mpa pressure, 9 surface of substrate work-piece is flowed to from spray head 5.
Step 3: after setting arc track and the speed of travel of the walking of anode tool-electrode 4 in industrial personal computer 1, opening
High frequency pulse power supply is adjusted to constant pressure 6V, the electric current between 1 real-time detection anode tool-electrode 4 of industrial personal computer and the electrode of preparation
Variation, when the electrode of generation and 4 spacing of anode tool-electrode are too small, electric current increases, when being more than set threshold current,
Control three-dimensional mobile platform is lifted along z-axis, so that electric current maintains always setting value, to guarantee anode tool-electrode 4 and structure
Suitable interpolar is maintained between part away from (between 0.1-1mm).
Step 4: after electrode growth reaches specified size, stop high frequency pulse power supply power supply, stops chemical pump 2 and work,
Substrate work-piece 9 is taken out, flattens use after cutting the electrode of generation.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (7)
1. a kind of dendrite nickel catalyst electrode preparation facilities based on 3D printing, which is characterized in that including industrial personal computer (1), chemical industry
Pump (2), anode tool-electrode (4), plating solution spray head (5), connector (7), coating bath (8), three-dimensional mobile platform (10)；Industrial personal computer
(1) it is used as three-dimensional motion control system, the modeling graph data of the nickel catalyst electrode for receiving user is automatically converted into three
The motion control data of mobile platform is tieed up, for controlling three-dimensional mobile platform in X, Y, Z-direction movement；
Plating solution spray head (5) includes guide pipe (11), perforated baffle (15), nozzle housing body (16)；Wherein nozzle housing body (16)
For the consistent cylindrical shape of internal diameter, plating solution sprays vertically downward, can form pine-tree structure in electrode surface；Nozzle housing body (16)
Upper end is fixed with guide pipe (11), and guide pipe (11) passes through for sealing with clamping anode tool-electrode (4), perforated baffle (15)
Interference connection is mounted on anode tool-electrode (4), and load has alloying metal particle (14) on perforated baffle, passes through alloying metal
Grain (14) supplements the ion consumed in plating solution；Be provided with through-hole in the outer surface on nozzle housing body (16) top, the hole with
Emulsion tube (3) one end is connected, then emulsion tube (3) other end is connected with chemical pump (2) entrance, and chemical pump (2) outlet is passed through
Coating bath (8) realizes that plating solution circulates in coating bath；After opening chemical pump (2), plating solution flows vertically downward from plating solution spray head
Out；
Substrate work-piece (9) is lain in coating bath (8), and anode tool-electrode (4) is filled together with plating solution spray head (5) by connector (7)
It is clipped on three-dimensional mobile platform (10), three-dimensional mobile platform (10) drives anode tool-electrode (4) and plating solution spray head (5) in three-dimensional
It is moved in space；Anode tool-electrode (4) and substrate work-piece (9) connect respectively industrial personal computer (1) medium-high frequency pulse power anode and
Cathode drives anode tool-electrode (4) and plating solution spray head (5) root through three-dimensional mobile platform (10) under the control of industrial personal computer
It is moved according to the motion control data of three-dimensional mobile platform along the track of setting.
2. dendrite nickel catalyst electrode preparation facilities according to claim 1, which is characterized in that anode tool-electrode (4)
With curvature, curvature is identical as pre-prepared dendrite nickel catalyst electrode skeleton curvature, under being guided by anode tool-electrode
Local plating effect, deposits nickel catalyst electrode identical with anode shape.
3. dendrite nickel catalyst electrode preparation facilities according to claim 1, which is characterized in that industrial personal computer (1) is according to right
The current value real-time monitoring of high frequency pulse power supply constantly adjusts anode tool-electrode (4) height, makes anode tool-electrode and preparation
Electrode spacing position keep constant.
4. the method that -3 any described devices prepare dendrite nickel catalyst electrode according to claim 1, which is characterized in that
Step (1): substrate work-piece (9) is laid flat into coating bath (8), selects the anode tool-electrode for being suitble to curvature as needed
(4), and with plating solution spray head (5) it is connected, anode tool-electrode (4) exposes outside nozzle mouth 0.5cm, is being fixed to three-dimensional
On the connector (7) of mobile platform (10)；
Step (2): by industrial personal computer (1) medium-high frequency pulse power anode and cathode respectively with anode tool-electrode (4) and matrix work
Part (9) is connected, and three-dimensional mobile platform z-axis coordinate is adjusted, so that anode tool-electrode (4) and substrate work-piece (9) surface are between 1mm
Every；The inlet of chemical pump (2) is connected with coating bath (8) again, outlet is connected with two inlet of outside of plating solution spray head (5), opens
Chemical pump (2) are opened, so that flowing to substrate work-piece (9) surface from spray head (5) after plating solution reaches 0.1Mpa pressure；
Step (3): importing the modeling graph data of the nickel catalyst electrode of user in industrial personal computer (1), opens high-frequency electrical pulses
Source, industrial personal computer (1) real-time detection anode tool-electrode (4) and preparation electrode between curent change, when generation electrode with
When anode tool-electrode (4) spacing is too small, electric current increases, and when being more than set threshold current, controls three-dimensional mobile platform
It is lifted along z-axis, so that electric current maintains always setting value, to guarantee to maintain conjunction between anode tool-electrode (4) and component
Suitable interpolar away from.
Step (4): after electrode growth reaches specified size, stopping high frequency pulse power supply power supply, stop chemical pump (2) work,
Substrate work-piece (9) are taken out, flatten use after cutting the electrode of generation.
5. according to the method described in claim 4, it is characterized in that, high frequency pulse power supply output voltage is constant pressure 6V.
6. according to the method described in claim 4, it is characterized in that, suitable interpolar between anode tool-electrode (4) and component
Away between 0.1-1mm.
7. according to the method described in claim 4, it is characterized in that, plating solution uses: the nickel sulfate of 300g/l, the chlorination of 40g/l
The boric acid of nickel and 40g/l；Boric acid and 990mL distilled water are successively first poured into beaker, 70-90 DEG C of heating water bath simultaneously uses glass bar
Stirring dissolves boric acid；It is subsequently poured into nickel sulfate and nickel chloride, continue heating water bath and is stirred with glass bar to whole dissolutions；?
Enter active carbon particle and hydrogen peroxide reagent activation 30min, and is filtered for use with filter paper；Remaining 10mL is poured into another beaker
Distilled water, with homogenizer with 600-700r/min revolving speed stir 10min, stand it is stand-by to room temperature.
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| CN201910159965.8A CN109825856B (en) | 2019-03-04 | 2019-03-04 | Dendritic crystal nickel-based catalytic electrode preparation device and method based on 3D printing |
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| CN201910159965.8A CN109825856B (en) | 2019-03-04 | 2019-03-04 | Dendritic crystal nickel-based catalytic electrode preparation device and method based on 3D printing |
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| CN111575768A (en) * | 2020-05-25 | 2020-08-25 | 吉林大学 | Ceramic metal composite material dual-mode additive manufacturing device and printing method |
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| CN111575768B (en) * | 2020-05-25 | 2022-02-01 | 吉林大学 | Ceramic metal composite material dual-mode additive manufacturing device and printing method |
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| CN109825856B (en) | 2021-04-02 |
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